EP2089130B1 - Installation for the distillation of alcohol, especially ethyl alcohol, from fermented mash - Google Patents

Installation for the distillation of alcohol, especially ethyl alcohol, from fermented mash Download PDF

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Publication number
EP2089130B1
EP2089130B1 EP07819126.9A EP07819126A EP2089130B1 EP 2089130 B1 EP2089130 B1 EP 2089130B1 EP 07819126 A EP07819126 A EP 07819126A EP 2089130 B1 EP2089130 B1 EP 2089130B1
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EP
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Prior art keywords
column
alcohol
reboiler
distillation
distillation column
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EP07819126.9A
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German (de)
French (fr)
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EP2089130A1 (en
Inventor
Daniel Bethge
Paul Hildenbrand
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GEA Wiegand GmbH
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GEA Wiegand GmbH
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/001—Processes specially adapted for distillation or rectification of fermented solutions
    • B01D3/003—Rectification of spirit
    • B01D3/004—Rectification of spirit by continuous methods
    • B01D3/005—Combined distillation and rectification
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/36—Azeotropic distillation
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the invention relates to a plant for distilling alcohol, in particular ethyl alcohol from fermented mash.
  • ethyl alcohol is also suitable as a fuel for driving internal combustion engines.
  • the conventional production of ethyl alcohol from renewable agricultural raw materials requires relatively high energy consumption.
  • the alcohol is made from fermented, i. fermented and thus alcohol containing mash by means of a distillation column, also called mash column, expelled. Since the alcohol concentration of the raw alcohol expelled in the distillation column is comparatively low, the alcohol concentration in a subsequent rectification column and optionally a dehydrogenation process must be increased to a value sufficient for its later use as a fuel or industrial alcohol.
  • the energy requirement of the distillation plant is determined to a greater extent by the energy requirement of the rectification column, which is usually heated by live steam.
  • the distillation column can in turn be energy-saving by recovering the heat energy, for example, the Kopfbrüdens the rectification column, heated.
  • US 4,511,437 A is a plant for distilling alcohol with three distilling the alcohol from fermented mash distillation columns known to work parallel to each other with respect to the alcohol product stream and give raw alcohol together to two again alcohol product side parallel rectification columns. Energetically, the columns are connected in series, with the head vapors of the individual columns each heating a reboiler of a lower pressure column in each case arranged column.
  • a plant for distilling alcohol which in each case comprises two column pairs consisting of a distillation column and a rectification column.
  • the distillation column of each column pair withdraws from fermented, alcoholic mash raw alcohol and leads resulting, alcoholic Kopfbrüden the foot of each associated rectification column.
  • the head vapors of the two rectification columns condenses in top condensers, wherein a portion of the head vapor condensate of the respective rectification column is in turn supplied as a head-side reflux.
  • a portion of the head broth of the rectification column of the first column pair also heats a reboiler of the rectification column of the second column pair.
  • a distillation plant which allows to disassemble a multi-fuel system with at least three components in its individual components.
  • the plant comprises several distillation columns whose subregions are connected in series, taking into account different volatility of the components via two-way connections and / or one-way connections based on the product route.
  • the multi-material product is thus broken down successively into partial products with a reduced number of components and subsequently into individual components.
  • the invention is based on a plant for distilling alcohol, in particular ethyl alcohol from fermented mash, the at least one of the fermented mash raw alcohol stripping distillation column and one of the distillation column downstream, the alcohol concentration comprising increasing rectification column.
  • the improvement according to the invention consists in that the at least one distillation column is followed by a rectifying column concentrating the crude alcohol of the distillation column, whose head vapor condensate can be fed to the rectification column as head-side reflux and from whose foot region alcohol-water mixture of the rectification column can be fed as feed to be concentrated, the head vapor the amplification column is used to heat the distillation column, wherein the reboiler of the distillation column heated by the head vapor also forms the condenser of the amplification column, and wherein the rectification column is followed by a molecular sieve arrangement for dehydrogenating the rectified alcohol.
  • the Kopfbrüden the amplifier column already consists of rectified alcohol. Due to the alcohol content in the foot region of the reinforcing column, the temperature difference to the top of the column is low.
  • the reinforcing column can therefore be easily integrated into the heat balance of the distillation unit, i. heat by the energy of product streams from other stages of the distillation plant.
  • ethanol is rectified to the azeotropic point, ie a concentration of about 96% by volume in the final product. It has been shown that for use as a fuel or industrial alcohol, rectification is only sufficient up to about 94% by volume, especially if the ethyl alcohol concentrated in this way is dehydrated in a subsequent stage, in particular a molecular sieve arrangement.
  • the energy requirement of the distillation unit can be considerably reduced by limiting the rectification to an alcohol concentration of about 94% by volume, especially if at the same time it is ensured that the distillation temperature of the distillation column is kept below 85 ° C.
  • the distillation column subtracts the crude alcohol at a distillation temperature of less than 85 ° C and the rectification column increases the alcohol concentration of the crude alcohol to about 94 vol%.
  • a distillation temperature of less than 85 ° C is suitable especially for mash raw materials with a relatively high protein content, as is the case for example with rye, wheat, barley, etc. If, owing to the lower concentration in the rectification column, secondary constituents remain in the final alcohol product, this is tolerable in the intended use for fuel or industrial alcohol.
  • the rectification column is followed by a molecular sieve arrangement for the dehydrogenation of the rectified alcohol.
  • the rectification column is expediently operated with head overpressure, for example of up to 3 bar, so that the rectified alcohol obtained in the rectification column in the molecular sieve arrangement can already be supplied in vapor form.
  • the rectified alcohol can be fed to the molecular sieve arrangement via a superheater, for example a superheater heated with live steam.
  • the heat content of the dehydrogenated in the molecular sieve arrangement alcohol can be used for the improvement of the heat balance of the distillation plant when a reboiler heating the reinforcing column is heated by the dehydrated alcohol.
  • the molecular sieve assembly has at least two molecular sieves alternately in a drying mode in which the rectified alcohol is dehydrated at elevated pressure and a regeneration mode in which the molecular sieve is rinsed with dehydrated alcohol at reduced pressure, rewetting that portion of the dehydrated alcohol ,
  • the molecular sieve operated in the drying mode discharges the dehydrogenated alcohol via the reboiler of the reinforcing column, while the other molecular sieve operated in regeneration mode absorbs a portion of the dehydrated alcohol and the alcohol moistened in the process via a condenser condensing the humidified alcohol a heated with live steam evaporator, in particular falling film evaporator of the rectification column as to feeding rectifying feed.
  • the energy requirement of the dehydrogenated in the molecular sieve arrangement alcohol is usually not enough to heat the reinforcing column.
  • the reinforcing column is heated by a further reboiler, which in turn is heated by Kopfbrüden the rectification column.
  • a reboiler associated with the rectification column is in turn heated by live steam in order to be able to cover the energy requirement of the rectification column.
  • the or the reboiler of the reinforcing column or / and the reboiler of the rectification column are expediently designed as arranged in a forced circulation evaporator.
  • Falling film evaporators are preferably used for this purpose, since they are distinguished by a comparatively low temperature difference between the heating temperature and the evaporation temperature.
  • the forced circulation loop of the reboiler of the reinforcing column is guided here by its foot region, wherein the alcohol inflow of the rectification column is branched off from this forced circulation loop.
  • the condensate of the reboiler of the distillation column and / or the reboiler of the reinforcing column is advantageously fed to the reinforcing column or / and the rectification column as reflux.
  • the heated by dehydrated alcohol reboiler of the reinforcing column condenses the dehydrated alcohol usually not completely.
  • the heat content of the dehydrated alcohol can be used to preheat the condensed alcohol-water mixture as it leaves the condenser in the regeneration mode of the molecular sieve assembly.
  • the head vapor of the reinforcing column is used to heat the distillation column.
  • the heated by the Kopfbrüden Reboiler of the distillation column also forms the condenser of the reinforcing column, wherein the condensate of the overhead vapor of the reinforcing column and / or the rectification column can be fed as reflux.
  • the condensate of the reboiler heated by head vapor of the rectification column can also be fed as reflux to the reinforcing column of this or / and the rectification column.
  • the alcohol concentration Column or steam-heated reboiler is assigned and at least a portion of the thin juice fraction is passed into a forced circulation loop through the falling film evaporator, and at least some of the thin juice fraction or vapors circulating in the forced circulation circuit can be supplied to the distillation column for heating thereof.
  • the falling film evaporator used as reboiler of the distillation column can be easily integrated into the energy balance of the distillation unit.
  • the solids fraction of the vinasse is separated in the separator, for example, designed as a decanter and only the thin juice fraction circulated through the forced circulation, the pollution of the seepage-sensitive falling film evaporator is largely avoided.
  • the separated solids fraction is removed from the process. Conveniently, the vapor generated in the falling film evaporator is fed directly into the distillation column for heating.
  • the falling film evaporator forming the reboiler of the distillation column is heated by the reinforcing column arranged in the alcohol product stream between the distillation column and the rectification column and increasing the alcohol concentration of the crude alcohol. While this recovers some of the energy used to heat the boost column, this energy may not be enough to fully heat the distillation column after the boost column is operated at a lower energy level as compared to a conventional rectification column. In individual cases, therefore, the energy requirement of the distillation column must be supplemented elsewhere.
  • a forced circulation evaporator can be provided in a manner known per se, which is heated by overhead vapors of the distillation column. Since the pressure and the temperature of the top of the distillation column of the distillation column for the operation of the forced circulation evaporator is not sufficient, it is known to increase the pressure and the temperature of the Kopfbrüdens by means of a compressor. Since the compressor compresses vapors containing alcohol, the compressor must be explosion-proof, which considerably reduces the design effort elevated.
  • the Rohalkoholbrüden the distillation column is at least partially condensable in an evaporator used for the production of steam and the steam over a the pressure and / or the temperature of the water vapor increasing mechanical compressor of the distillation column or another, from the fermented mash can be fed as raw alcohol-withdrawing distillation column to the heating thereof.
  • the compressor thus compresses non-alcoholic water vapor and thus does not have to be explosion-proof. Since it is a mechanical compressor, it can be driven electrically, which can be relatively easily and inexpensively.
  • the energy requirement of the distillation column can be supplemented in this way, without the energy content of the overhead vapor of the reinforcing column or any other stage of the distillation would have to be increased only from the viewpoint of heating the distillation column.
  • the compressed by means of the mechanical compressor water vapor can be additionally supplied to the already partially heated by the reboiler distillation column.
  • a first distillation column can be heated by head vapor of a subsequent column increasing the alcohol concentration, for example the amplification column or rectification column, while the second distillation column is heated by the compressed water vapor of the mechanical compressor.
  • the two distillation columns, the mash is fed in parallel, but the second distillation column is preferably operated at a lower head temperature and lower pressure than the first distillation column.
  • the vapor-generating evaporator is preferably a falling-film evaporator in order to be able to use the low temperature difference between heating temperature and evaporation temperature in the case of the falling-film evaporator.
  • the falling-film evaporator is expediently arranged for the generation of the steam in a circulation circuit for fresh water or stillage or vapors.
  • the generation of steam from vinasse or vinasse has the advantage that the steam has sufficient temperature, since the vinasse is withdrawn from the heated foot region of the distillation column. If fresh water is used, it must be preheated. However, the use of fresh water avoids that components contained in the vinasse are transformed by cracking reactions in volatile substances that can reach the raw alcohol. The use of fresh water minimizes denaturation reactions and deposits in the falling film evaporator.
  • the mechanical compressor is nevertheless preferably connected to the circulation circuit via a separator separating the steam, in particular a flash separator.
  • the mechanical compressor may be constructed as a compressor or as a paddle wheel compressor. It is understood that the compressor may also include a plurality of serially connected mechanical compressor stages.
  • FIG. 1 shows a schematic diagram of an ethyl alcohol from fermented mash-producing distillation plant.
  • the distilling plant suitable for the production of ethyl alcohol as a fuel for internal combustion engines or for industrial purposes is fermented from a precursor 1 of the alcohol production process, ie fermented and thus ethyl alcohol-containing mash of a relatively high-protein agricultural raw material, such as rye, wheat, Barley, etc. supplied.
  • the mash is heated in a preheater 3 to the distillation temperature of a distillation column 5 and fed to the distillation column 5 via a line 7.
  • the head region, often also referred to as mashing column distillation column 5 is indicated at 11, her foot at 13.
  • the crude alcohol withdrawn from the head region 11 of the distillation column 5 as alcohol vapors is condensed in a multistage and at the same time energy recovery of the thermal energy contained in the crude alcohol and condensed in liquid form by means of a feed pump 17 via a raw alcohol to the rectification temperature of a booster column 19 Preheater 21 fed at 23 as an inlet.
  • the reinforcing column 19 already increases the alcohol content of the crude alcohol of the distillation column in the head to about 94% by volume; the remaining ethanol in the bottom is separated from the lutter water in the rectification column 33.
  • the rectified alcohol vapor withdrawn from the head region 25 of the amplification column 19 is, as will be explained in more detail below, condensed in a reboiler 27 which heats the distillation column 5 and used as a top condenser of the amplification column 19 and by means of a feed pump 29 both to the head region 25 of the amplification column 19 also fed to the head region 31 of a rectification column 33 connected downstream of the amplification column 19 as reflux.
  • the feed of the rectification column 33 is ethanol-water mixture, which is withdrawn via a forced circulation circuit 35 by means of a feed pump 37 from the foot region 39 of the reinforcing column 19 and fed via a line 41 of the rectification column 33.
  • ethyl alcohol is dehydrated in a molecular sieve assembly 43 and is available as a rectified and dehydrated ethyl alcohol at 45 as an end product.
  • the energy requirement of the distillation plant is determined primarily by the energy requirement of the concentration and less by the removal of raw alcohol from the mash.
  • the rectification takes place in two stages, i. In the booster column 19 and the rectification column 33. Since the reflux of the rectification column 33 is taken from the top product of the booster column 19 and the inflow of the rectification column 33 to the bottom portion 39 of the booster column 19, the temperature difference of the base portion 39 to the top portion 25 of the booster column 19 is comparatively low. so that the reinforcing column 19 can be well integrated into the heat balance of the distillation still even if the rectification column 33 is operated only at a head temperature between 85 and 110 ° C.
  • the rectification column 33 only concentrates the alcohol to about 94% by volume before the rectified alcohol is fed to the molecular sieve arrangement 43 for dehydrogenation.
  • the distillation temperature of the distillation column 5 is limited to a temperature of less than 85 ° C, so that the distillation process is carried out at a lower energy level than before.
  • the reboiler 27 which is heated by head vapor of the amplification column 19 and condenses the head vapor is designed as a falling film evaporator and heats the foot region 13 of the distillation column 5.
  • the non-alcoholic stillage obtained in the distillation column 5 is fed via a foot region outlet 49 to a decanter 51 which separates the vinasse into a at 53 removed from the process solids fraction and a via a line 54 downstream of the reboiler 27 but before a feed pump 56 into the forced circulation 47 split thin juice fraction divided.
  • the forced circulation circuit 47 does not circulate the still, but rather the thin juice fraction which is largely freed of solids.
  • the vinasse is withdrawn at a lowermost located in the foot area 13 point. It is understood that the vinasse can also be withdrawn at an overlying location, for example in the region of the lowest bottom of the distillation column 5, so that the forced circulation circuit 47 carrying the thin juice fraction can if necessary also run directly through the foot region 13.
  • the condenser assembly 15 condensing the crude alcohol vapors from the head region 11 of the distillation column 5 comprises, as a first stage, a falling-film evaporator 55 for generating low-pressure steam which is discharged to a mechanical compressor 59 via an expansion gravity separator 57.
  • the mechanical compressor 59 increases the pressure and the temperature of the water vapor and blows the compressed steam directly into the foot region 13 for additional heating of the distillation column 5. In this way, a portion of the heat of condensation of the crude alcohol overheads of the distillation column 5 is recovered for the heating of the distillation column. Since the mechanical compressor 59, unlike conventional vapor compressors, does not compress alcohol vapor but water vapor, the compressor 59 does not have to be explosion-proof.
  • the falling-film evaporator 55 is disposed in a forced circulation circuit 63 provided with a pump 61, and evaporates in the forced circulation circuit circulating fresh water which is supplied at 65 from a source, not shown, in preheated form. From the forced circulation circuit 47 downstream of the pump 56 running thin juice fraction or Dünnschlempe is supplied via the separator 57 to the forced circulation circuit 63 of the falling film evaporator 55 in addition to the fresh water supply and leaves the forced circulation circuit 63 and thus the process at 67.
  • the low-pressure steam has on the input side of the compressor 59, a pressure of for example about 200 to 250 mbar and is raised by the compressor 59 to an outlet pressure between 500 and 600 mbar at a temperature between 70 and 90 ° C.
  • the mechanical compressor can be designed as a single-stage or as a multi-stage compressor. Suitable are rotating compressors, but also bucket wheel compressors or Ventillatoren. Since the compressor 59 is driven by an electric motor, the drive energy can be made available more simply than is possible, for example, with a steam jet compressor.
  • the distillation column 5 expediently operates at a head temperature between 55 and 75 ° C and a top pressure between 300 and 500 mbar.
  • a falling film evaporator 55 instead of the falling film evaporator 55, another type of evaporator could also be used.
  • Advantage of the falling film evaporator is its low temperature difference of, for example, 5 ° C between the inlet temperature of the at least partially to be condensed Rohalkoholbrüdens the distillation column 5 and the outlet temperature of the low-pressure steam.
  • the compressor capacity of the compressor 59 can be reduced in this way.
  • the forced circulation circuit 63 fresh water is supplied, which reduces the risk of Denaturéessrevatien and secondary component formation. It is understood that it is also possible to work exclusively with thin juice fraction or thin still in the forced circulation circuit 63.
  • the uncondensed vapor fraction at 69 is fed to the preheater 3 for preheating the mash, forming the second stage of the condensation assembly 15.
  • the technicallybrüden of the preheater 3 is finally fed to a main capacitor 71, which forms the third stage of the condensation assembly 15 and the raw alcohol as liquid condensate via the feed pump 17 emits for forwarding to the reinforcing column 19.
  • the main condenser 71 is connected to a cooling water source 73 and is also connected to a vacuum pump 75, via which the negative pressure in the distillation unit is set.
  • the mash of the distillation column 5 is supplied near its top portion 11, so dispensed with a separate from the gain column 19 gain range. Accordingly, the raw alcohol leaving the main condenser 71 has a concentration of only 40 to 60% by volume. The energy requirement of the distillation column 5 is thus comparatively low.
  • the concentration of the crude alcohol takes place in the reinforcing column 19 and subsequently the rectification column 33. Since the rectification is distributed in two stages, can be worked here energetically favorable. It is understood, however, that also the distillation column 5 may to some extent comprise additional soils for concentration.
  • the reinforcing column 19 is heated primarily by a reboiler 77 designed as a falling-film evaporator, which at the same time forms the top condenser of the rectification column 33.
  • the reboiler 77 is connected to the forced circulation circuit 35 leading through the foot region 39 of the reinforcing column 19.
  • the rectification column 33 is heated in a similar manner primarily via a reboiler 79 designed as a falling-film evaporator, which is connected to a forced circulation circuit 83 guided through the foot region 81 of the rectification column 33.
  • a feed pump of the forced circulation circuit 83 is shown at 85.
  • the reboiler 79 is heated by live steam, which is supplied to it from a live steam source 87 via a line 89.
  • Lutter water circulating in the forced circulation circuit 83 from the foot region 81 is withdrawn downstream of the pump 85 via a line 91 and removed from the process at 93 after it has been utilized in the preheater 21 to preheat the crude liquid alcohol fed to the boost column 19.
  • the rectification column 33 comprises about 50 trays and provides the rectified alcohol at a pressure of about 1.5 to 6 bar, for example 2 bar, on a side draw 95 in vapor form at an alcohol concentration of about 94 vol %.
  • the vaporous, rectified alcohol is fed to a likewise heated from the live steam source 87 superheater 97, which supplies the superheated alcohol vapor at 99 of the molecular sieve assembly 43 for dehydration.
  • the molecular sieve arrangement 43 has, in a manner known per se, a plurality of molecular sieves, in this case three molecular sieves 101, 103 and 105, which in FIG cyclic permutation in each case in a drying mode and a regeneration mode.
  • a molecular sieve in this case the molecular sieve 101, operates in the drying mode, while the other two molecular sieves 103, 105 are switched into their regeneration mode.
  • the superheated vaporous alcohol is fed to the molecular sieve currently operating in the drying mode, here the molecular sieve 101, which delivers the dehydrated alcohol to a manifold 107 to which the molecular sieves 101, 103, 105 share their dehydrated alcohol exits are connected.
  • the regeneration mode molecular sieves 103, 105 are connected to a vacuum source 111 via a condenser 109 for regeneration mode operation, and the dehydrogenated alcohol fed back to the molecular sieves 103, 105 through the regenerated molecular sieves 103, 105 and through the dehydrated alcohol fed through the manifold 107 sucks the capacitor 109.
  • the condenser 109 is supplied with cooling water from the cooling water source 73 and condenses the alcohol-water vapor mixture rehydrated in the molecular sieves 103, 105 during regeneration.
  • a pump 113 conveys the alcohol-water mixture collecting in a collecting tank 115 in the process.
  • the number of molecular sieves may differ from the illustrated embodiment.
  • at least two molecular sieves are required, operating alternately in the drying mode and the regeneration mode. Since the regeneration mode may last longer than the dehydration usable drying cycle time, the number of molecular sieves operated in the regeneration mode is desirably greater than the number of molecular sieves operated in the drying mode.
  • the for the cyclical Exchange and switching of the molecular sieves required controllable connection lines are indicated at 117.
  • the resulting in the regeneration mode alcohol-water mixture is fed again to the rectification. Since the mixture was cooled in the condensation in the condenser 109 to a temperature of about 40 ° C, it is preheated in a preheater 119 and fed via a line 121 to a forced circulation circuit 123 of a here designed as a falling film evaporator evaporator 125. The evaporator 125 is likewise heated with live steam from the live steam source 87 and releases the mixture heated to the rectification temperature at 127 as feed to the rectification column 33. A feed pump of the forced circulation circuit 123 is shown at 129.
  • the alcohol dehydrogenated in the molecular sieve arrangement 43 heats a further reboiler 139, formed as a falling-film evaporator, of the booster column 19, which is connected in parallel to the reboiler 77 to the forced circulation circuit 35.
  • the dehydrated alcohol is supplied to the reboiler 139 from the manifold 107 and fed via a feed pump 141 to the preheater 119 for preheating the alcohol-water mixture obtained in the regeneration mode of the molecular sieve assembly 43, to finally be withdrawn at 45 as the final product.
  • the reboiler 27 of the distillation column 5 also forms the top condenser of the reinforcing column 19, while the reboiler 77 of the reinforcing column 19 at the same time forms the top condenser of the rectification column 33.
  • the alcohol condensate obtained in the reboilers 27 and 77 at 143 and 145, respectively, is conveyed by the feed pump 29 147 of the reinforcing column and fed at 149 of the rectification column in the head region as reflux.
  • Fusel oil accumulating in the rectification process is withdrawn at 151 from the boost column and at 153 from the rectification column and removed from the process at 155.
  • the above-described distillation plant allows to distill ethyl alcohol from wheat, rye, etc. in a low-temperature process. While conventional plants require about 2 kg of heating steam per liter of pure alcohol, corresponding to about 4000 kJ per liter of pure alcohol, the distilling plant according to the invention requires only about 2300 kJ per liter of pure alcohol plus about 54 W per liter of pure alcohol in electrical energy for the vapor compression.

Description

Die Erfindung betrifft eine Anlage zum Destillieren von Alkohol, insbesondere Ethylalkohol aus fermentierter Maische.The invention relates to a plant for distilling alcohol, in particular ethyl alcohol from fermented mash.

Neben Benzin und Dieselöl eignet sich auch Ethylalkohol als Kraftstoff für den Antrieb von Brennkraftmaschinen. Allerdings bedingt die herkömmliche Herstellung von Ethylalkohol aus nachwachsenden Agrarrohstoffen einen relativ hohen Energieverbrauch. In einer herkömmlichen Destillieranlage wird der Alkohol aus fermentierter, d.h. vergorener und damit Alkohol enthaltender Maische mittels einer Destillationskolonne, auch Maischekolonne genannt, ausgetrieben. Da die Alkoholkonzentration des in der Destillationskolonne ausgetriebenen Rohalkohols vergleichsweise niedrig ist, muss die Alkoholkonzentration in einer nachfolgenden Rektifikationskolonne und ggf. einem Dehydrierungsprozess auf einen seiner späteren Verwendung als Kraftstoff oder Industriealkohol genügenden Wert erhöht werden.Apart from gasoline and diesel oil, ethyl alcohol is also suitable as a fuel for driving internal combustion engines. However, the conventional production of ethyl alcohol from renewable agricultural raw materials requires relatively high energy consumption. In a conventional distillation plant, the alcohol is made from fermented, i. fermented and thus alcohol containing mash by means of a distillation column, also called mash column, expelled. Since the alcohol concentration of the raw alcohol expelled in the distillation column is comparatively low, the alcohol concentration in a subsequent rectification column and optionally a dehydrogenation process must be increased to a value sufficient for its later use as a fuel or industrial alcohol.

Der Energiebedarf der Destillieranlage wird zum größeren Teil durch den Energiebedarf der Rektifikationskolonne bestimmt, die üblicherweise durch Frischdampf beheizt wird. Die Destillationskolonne kann ihrerseits energiesparend durch Rückgewinnen der Wärmeenergie, beispielsweise des Kopfbrüdens der Rektifikationskolonne, beheizt werden.The energy requirement of the distillation plant is determined to a greater extent by the energy requirement of the rectification column, which is usually heated by live steam. The distillation column can in turn be energy-saving by recovering the heat energy, for example, the Kopfbrüdens the rectification column, heated.

Aus US 4,511,437 A ist eine Anlage zum Destillieren von Alkohol mit drei den Alkohol aus fermentierter Maische abziehenden Destillationskolonnen bekannt, die bezüglich des Alkoholproduktstroms zueinander parallel arbeiten und Rohalkohol gemeinsam an zwei wiederum alkoholproduktseitig parallel geschaltete Rektifikationskolonnen abgeben. Energetisch sind die Kolonnen in Reihe geschaltet, wobei der Kopfbrüden der einzelnen Kolonnen jeweils einen Reboiler einer im Druckniveau jeweils niedriger angeordneten Kolonne heizt.Out US 4,511,437 A is a plant for distilling alcohol with three distilling the alcohol from fermented mash distillation columns known to work parallel to each other with respect to the alcohol product stream and give raw alcohol together to two again alcohol product side parallel rectification columns. Energetically, the columns are connected in series, with the head vapors of the individual columns each heating a reboiler of a lower pressure column in each case arranged column.

Aus WO 88/02649 A1 ist eine Anlage zum Destillieren von Alkohol bekannt, die jeweils zwei aus einer Destillationskolonne und einer Rektifikationskolonne bestehende Kolonnenpaare umfasst. Die Destillationskolonne jedes Kolonnenpaars zieht aus vergorener, alkoholhaltiger Maische Rohalkohol ab und führt entstehenden, alkoholhaltigen Kopfbrüden dem Fußbereich der jeweils zugeordneten Rektifikationskolonne zu. Der Kopfbrüden der beiden Rektifikationskolonnen kondensiert in Kopfkondensatoren, wobei ein Teil des Kopfbrüdenkondensats der jeweiligen Rektifikationskolonne wiederum als kopfseitiger Rücklauf zugeführt wird. Ein Anteil des Kopfbrüdens der Rektifikationskolonne des ersten Kolonnenpaars heizt darüber hinaus einen Reboiler der Rektifikationskolonne des zweiten Kolonnenpaars. In einer Variante der aus WO 88/02649 A1 bekannten Destillieranlage ist zusätzlich zu den beiden Kolonnenpaaren ein Kondensatstripper vorgesehen, dem aus den Fußbereichen der beiden Rektifikationskolonnen wie auch aus dem Reboiler der Destillationskolonne des zweiten Kolonnenpaars Kondensat kopfseitig zugeführt wird.Out WO 88/02649 A1 For example, a plant for distilling alcohol is known, which in each case comprises two column pairs consisting of a distillation column and a rectification column. The distillation column of each column pair withdraws from fermented, alcoholic mash raw alcohol and leads resulting, alcoholic Kopfbrüden the foot of each associated rectification column. The head vapors of the two rectification columns condenses in top condensers, wherein a portion of the head vapor condensate of the respective rectification column is in turn supplied as a head-side reflux. A portion of the head broth of the rectification column of the first column pair also heats a reboiler of the rectification column of the second column pair. In a variant of the WO 88/02649 A1 known distilling a condensate stripper is provided in addition to the two column pairs, which is fed from the foot of the two rectification columns as well as from the reboiler of the distillation column of the second column pair condensate on the head side.

Aus EP 1 080 766 A1 ist eine Destillieranlage bekannt, die es erlaubt, ein Mehrstoffsystem mit wenigstens drei Komponenten in seine Einzelkomponenten zu zerlegen. Die Anlage umfasst mehrere Destillationskolonnen, deren Teilbereiche unter Berücksichtigung unterschiedlicher Flüchtigkeit der Komponenten über Zwei-Wege-Verbindungen und/oder Ein-Weg-Verbindungen bezogen auf den Produktweg seriell miteinander verbunden sind. Das Mehrstoffprodukt wird auf diese Weise nacheinander in Teilprodukte mit verringerter Komponentenzahl und nachfolgend in Einzelkomponenten zerlegt.Out EP 1 080 766 A1 a distillation plant is known, which allows to disassemble a multi-fuel system with at least three components in its individual components. The plant comprises several distillation columns whose subregions are connected in series, taking into account different volatility of the components via two-way connections and / or one-way connections based on the product route. The multi-material product is thus broken down successively into partial products with a reduced number of components and subsequently into individual components.

Es ist Aufgabe der Erfindung, eine Destillieranlage für aus nachwachsenden Agrarrohstoffen hergestellten Alkohol, insbesondere Ethylalkohol anzugeben, die mit weniger Betriebsenergie als bisher auskommt.It is an object of the invention to provide a distillation plant for alcohol produced from renewable agricultural raw materials, in particular ethyl alcohol, which manages with less operating energy than before.

Die Erfindung geht von einer Anlage zum Destillieren von Alkohol, insbesondere Ethylalkohol aus fermentierter Maische aus, die wenigstens eine aus der fermentierten Maische Rohalkohol abziehende Destillationskolonne und einer der Destillationskolonne nachgeschaltete, die Alkoholkonzentration erhöhende Rektifikationskolonne umfasst. Die erfindungsgemäße Verbesserung besteht darin, dass der wenigstens einen Destillationskolonne eine den Rohalkohol der Destillationskolonne aufkonzentrierende Verstärkungskolonne nachgeschaltet ist, deren Kopfbrüdenkondensat der Rektifikationskolonne als kopfseitiger Rücklauf zuführbar ist und aus deren Fußbereich Alkohol-Wasser-Gemisch der Rektifikationskolonne als aufzukonzentrierender Zulauf zuführbar ist, wobei der Kopfbrüden der Verstärkungskolonne zur Beheizung der Destillationskolonne genutzt wird, wobei der durch den Kopfbrüden beheizte Reboiler der Destillationskolonne zugleich den Kondensator der Verstärkungskolonne bildet,und wobei der Rektifikationskolonne eine Molekularsiebanordnung zur Dehydrierung des rektifizierten Alkohols nachgeschaltet ist.The invention is based on a plant for distilling alcohol, in particular ethyl alcohol from fermented mash, the at least one of the fermented mash raw alcohol stripping distillation column and one of the distillation column downstream, the alcohol concentration comprising increasing rectification column. The improvement according to the invention consists in that the at least one distillation column is followed by a rectifying column concentrating the crude alcohol of the distillation column, whose head vapor condensate can be fed to the rectification column as head-side reflux and from whose foot region alcohol-water mixture of the rectification column can be fed as feed to be concentrated, the head vapor the amplification column is used to heat the distillation column, wherein the reboiler of the distillation column heated by the head vapor also forms the condenser of the amplification column, and wherein the rectification column is followed by a molecular sieve arrangement for dehydrogenating the rectified alcohol.

Der Kopfbrüden der Verstärkerungskolonne besteht bereits aus rektifiziertem Alkohol. Auf Grund des Alkoholgehalts im Fußbereich der Verstärkungskolonne ist die Temperaturdifferenz zum Kolonnenkopf gering. Die Verstärkungskolonne lässt sich deshalb problemlos in den Wärmehaushalt der Destillieranlage integrieren, d.h. durch die Energie von Produktströmen anderer Stufen der Destillieranlage beheizen.The Kopfbrüden the amplifier column already consists of rectified alcohol. Due to the alcohol content in the foot region of the reinforcing column, the temperature difference to the top of the column is low. The reinforcing column can therefore be easily integrated into the heat balance of the distillation unit, i. heat by the energy of product streams from other stages of the distillation plant.

Herkömmlich wird Ethanol bis zum azeotropen Punkt, d.h. einer Konzentration von etwa 96 Vol% im Endprodukt rektifiziert. Es hat sich gezeigt, dass für die Nutzung als Kraftstoff oder Industriealkohol eine Rektifikation lediglich bis etwa 94 Vol% hinreichend ist, insbesondere wenn der solchermaßen aufkonzentrierte Ethylalkohol in einer nachfolgenden Stufe, insbesondere einer Molekularsiebanordnung dehydriert wird. Der Energiebedarf der Destillieranlage kann durch Begrenzen der Rektifikation auf eine Alkoholkonzentration von etwa 94 Vol% beträchtlich verringert werden, insbesondere wenn zugleich dafür gesorgt wird, dass die Destillationstemperatur der Destillationskolonne unter 85°C gehalten wird. Der Energiebedarf der Destillationskolonne wird auf diese Weise gleichfalls verringert und kann zu einem wesentlichen Teil aus dem Energieabfluss insbesondere der Rektifikationskolonne gedeckt werden. In einer bevorzugten Ausgestaltung ist deshalb vorgesehen, dass die Destillationskolonne den Rohalkohol bei einer Destillationstemperatur von weniger als 85°C abzieht und die Rektifikationskolonne die Alkoholkonzentration des Rohalkohols auf etwa 94 Vol% erhöht. Eine Destillationstemperatur von weniger als 85°C eignet sich
insbesondere für Maischerohstoffe mit einem relativ hohen Proteinanteil, wie dies zum Beispiel bei Roggen, Weizen, Gerste usw. der Fall ist. Sollten auf Grund der geringeren Aufkonzentrierung in der Rektifikationskolonne Nebenbestandteile in dem Alkohol-Endprodukt bleiben, so ist dies bei der vorgesehenen Verwendung für Kraftstoff oder Industriealkohol tolerabel.Traditionally, ethanol is rectified to the azeotropic point, ie a concentration of about 96% by volume in the final product. It has been shown that for use as a fuel or industrial alcohol, rectification is only sufficient up to about 94% by volume, especially if the ethyl alcohol concentrated in this way is dehydrated in a subsequent stage, in particular a molecular sieve arrangement. The energy requirement of the distillation unit can be considerably reduced by limiting the rectification to an alcohol concentration of about 94% by volume, especially if at the same time it is ensured that the distillation temperature of the distillation column is kept below 85 ° C. The energy requirement of the distillation column is also reduced in this way and can be covered to a substantial extent from the energy effluent, in particular the rectification column. In a preferred embodiment, it is therefore provided that the distillation column subtracts the crude alcohol at a distillation temperature of less than 85 ° C and the rectification column increases the alcohol concentration of the crude alcohol to about 94 vol%. A distillation temperature of less than 85 ° C is suitable
especially for mash raw materials with a relatively high protein content, as is the case for example with rye, wheat, barley, etc. If, owing to the lower concentration in the rectification column, secondary constituents remain in the final alcohol product, this is tolerable in the intended use for fuel or industrial alcohol.

Erfindungsgemäß ist der Rektifikationskolonne eine Molekularsiebanordnung zur Dehydrierung des rektifizierten Alkohols nachgeschaltet. Die Rektifikationskolonne wird hierbei zweckmäßigerweise mit Kopfüberdruck, beispielsweise von bis zu 3 bar betrieben, so dass der in der Rektifikationskolonne dampfförmig anfallende rektifizierte Alkohol der Molekularsiebanordnung bereits in Dampfform zugeführt werden kann. Der rektifizierte Alkohol kann der Molekularsiebanordnung ggf. über einen Überhitzer, beispielsweise einem mit Frischdampf beheizten Überhitzer zugeführt werden.According to the invention, the rectification column is followed by a molecular sieve arrangement for the dehydrogenation of the rectified alcohol. The rectification column is expediently operated with head overpressure, for example of up to 3 bar, so that the rectified alcohol obtained in the rectification column in the molecular sieve arrangement can already be supplied in vapor form. If necessary, the rectified alcohol can be fed to the molecular sieve arrangement via a superheater, for example a superheater heated with live steam.

Der Wärmeinhalt des in der Molekularsiebanordnung dehydrierten Alkohols kann für die Verbesserung des Wärmehaushalts der Destillieranlage genutzt werden, wenn ein die Verstärkungskolonne beheizender Reboiler durch den dehydrierten Alkohol beheizt wird. Die Molekularsiebanordnung weist wenigstens zwei Molekularsiebe auf, die wechselweise in einem Trocknungsmodus, in welchem der rektifizierte Alkohol bei erhöhtem Druck dehydriert wird und einem Regenerationsmodus, in welchem das Molekularsieb bei erniedrigtem Druck mit dehydriertem Alkohol gespült wird, wobei dieser Anteil des dehydrierten Alkohols wieder befeuchtet wird. In einer bevorzugten Ausgestaltung ist vorgesehen, dass das im Trocknungsmodus betriebene Molekularsieb den dehydrierten Alkohol über den Reboiler der Verstärkungskolonne abgibt, während das andere, im Regenerationsmodus betriebene Molekularsieb einen Anteil des dehydrierten Alkohols aufnimmt und den hierbei befeuchteten Alkohol über einen den befeuchteten Alkohol kondensierenden Kondensator und einen mit Frischdampf beheizten Verdampfer, insbesondere Fallfilmverdampfer der Rektifikationskolonne als zu
rektifizierender Zulauf zuführt. Der im Regenerationsmodus befeuchtete, d.h. mit Wasser verdünnte Alkohol wird auf diese Weise erneut der Rektifikation zugeführt.The heat content of the dehydrogenated in the molecular sieve arrangement alcohol can be used for the improvement of the heat balance of the distillation plant when a reboiler heating the reinforcing column is heated by the dehydrated alcohol. The molecular sieve assembly has at least two molecular sieves alternately in a drying mode in which the rectified alcohol is dehydrated at elevated pressure and a regeneration mode in which the molecular sieve is rinsed with dehydrated alcohol at reduced pressure, rewetting that portion of the dehydrated alcohol , In a preferred embodiment, it is provided that the molecular sieve operated in the drying mode discharges the dehydrogenated alcohol via the reboiler of the reinforcing column, while the other molecular sieve operated in regeneration mode absorbs a portion of the dehydrated alcohol and the alcohol moistened in the process via a condenser condensing the humidified alcohol a heated with live steam evaporator, in particular falling film evaporator of the rectification column as to
feeding rectifying feed. The moistened in regeneration mode, ie diluted with water alcohol is fed to the rectification in this way again.

Der Energiebedarf des in der Molekularsiebanordnung dehydrierten Alkohols reicht in aller Regel nicht zur Beheizung der Verstärkungskolonne aus. In einer bevorzugten Ausgestaltung wird die Verstärkungskolonne durch einen weiteren Reboiler beheizt, der seinerseits durch Kopfbrüden der Rektifikationskolonne beheizt wird. Ein der Rektifikationskolonne zugeordneter Reboiler wird seinerseits durch Frischdampf beheizt, um den Energiebedarf der Rektifikationskolonne decken zu können. Der bzw. die Reboiler der Verstärkungskolonne oder/und der Reboiler der Rektifikationskolonne sind zweckmäßigerweise als in einem Zwangsumlaufkreis angeordnete Verdampfer ausgebildet. Bevorzugt werden hierzu Fallfilmverdampfer eingesetzt, da sich diese durch eine vergleichsweise niedrige Temperaturdifferenz zwischen Heiztemperatur und Verdampfungstemperatur auszeichnen. Der Zwangsumlaufkreis des Reboilers der Verstärkungskolonne ist hierbei durch deren Fußbereich geführt, wobei der Alkohol-Zufluss der Rektifikationskolonne aus diesem Zwangsumlaufkreis abgezweigt ist. Das Kondensat des Reboilers der Destillationskolonne oder/und des Reboilers der Verstärkungskolonne wird zweckmäßigerweise der Verstärkungskolonne oder/und der Rektifikationskolonne als Rückfluss zugeführt.The energy requirement of the dehydrogenated in the molecular sieve arrangement alcohol is usually not enough to heat the reinforcing column. In a preferred embodiment, the reinforcing column is heated by a further reboiler, which in turn is heated by Kopfbrüden the rectification column. A reboiler associated with the rectification column is in turn heated by live steam in order to be able to cover the energy requirement of the rectification column. The or the reboiler of the reinforcing column or / and the reboiler of the rectification column are expediently designed as arranged in a forced circulation evaporator. Falling film evaporators are preferably used for this purpose, since they are distinguished by a comparatively low temperature difference between the heating temperature and the evaporation temperature. The forced circulation loop of the reboiler of the reinforcing column is guided here by its foot region, wherein the alcohol inflow of the rectification column is branched off from this forced circulation loop. The condensate of the reboiler of the distillation column and / or the reboiler of the reinforcing column is advantageously fed to the reinforcing column or / and the rectification column as reflux.

Der durch dehydrierten Alkohol beheizte Reboiler der Verstärkungskolonne kondensiert den dehydrierten Alkohol in aller Regel nicht vollständig. Der Wärmeinhalt des dehydrierten Alkohols kann zur Vorwärmung des kondensierten Alkohol-Wasser-Gemisches genutzt werden, wie es im Regenerationsmodus der Molekularsiebanordnung deren Kondensator verlässt.The heated by dehydrated alcohol reboiler of the reinforcing column condenses the dehydrated alcohol usually not completely. The heat content of the dehydrated alcohol can be used to preheat the condensed alcohol-water mixture as it leaves the condenser in the regeneration mode of the molecular sieve assembly.

Der Kopfbrüden der Verstärkungskolonne wird zur Beheizung der Destillationskolonne ausgenutzt. Der durch den Kopfbrüden beheizte Reboiler der Destillationskolonne bildet zugleich den Kondensator der Verstärkungskolonne, wobei das Kondensat des Kopfbrüdens der Verstärkungskolonne oder/und der Rektifikationskolonne als Rückfluss zuführbar ist. In entsprechender Weise kann auch das Kondensat des durch Kopfbrüden der Rektifikationskolonne beheizten Reboilers der Verstärkungskolonne dieser oder/und der Rektifikationskolonne als Rücklauf zugeführt werden.The head vapor of the reinforcing column is used to heat the distillation column. The heated by the Kopfbrüden Reboiler of the distillation column also forms the condenser of the reinforcing column, wherein the condensate of the overhead vapor of the reinforcing column and / or the rectification column can be fed as reflux. In a corresponding manner, the condensate of the reboiler heated by head vapor of the rectification column can also be fed as reflux to the reinforcing column of this or / and the rectification column.

Es ist bekannt, die Destillationskolonne über einen als Zwangsumlaufverdampfer ausgebildeten Reboiler zu beheizen. Nachteilig bei diesem bekannten Reboiler ist, dass die im Zwangsumlaufverdampfer im Kreislauf geführte Schlempe überhitzt werden muss, was die Integrierung des Reboilers in den Energiehaushalt der Destillieranlage erschwert, denn der zur Beheizung des Reboilers beispielsweise aus einer anderen Prozessstufe zugeführte Brüden muss sich auf einen vergleichsweise hohen Temperaturniveau befinden, um eine Entspannungsverdampfung in der Destillationskolonne zu ermöglichen. Wird hingegen ein Fallfilmverdampfer eingesetzt, so erfolgt die Verdampfung anders als bei bisherigen Zwangsumlaufverdampfern nicht in der Destillationskolonne, sondern direkt in dem Reboiler. Das Produkt muss nicht für die Entspannungsverdampfung in der Destillationskolonne überhitzt werden und dementsprechend genügt eine vergleichsweise geringe Temperaturdifferenz zwischen der Heizseite und der Produktseite des Fallfilmverdampfers.It is known to heat the distillation column via a reboiler designed as a forced circulation evaporator. A disadvantage of this known reboiler is that the circulating in the forced circulation evaporator must be overheated, which complicates the integration of the reboiler in the energy balance of the distillation, because the supplied to heat the reboiler, for example, from another process stage vapors must be at a relatively high Temperature level to allow a flash evaporation in the distillation column. If, by contrast, a falling film evaporator is used, the evaporation takes place, unlike in previous forced circulation evaporators, not in the distillation column, but directly in the reboiler. The product need not be overheated for the flash evaporation in the distillation column, and accordingly, a comparatively small temperature difference between the heating side and the product side of the falling film evaporator is sufficient.

In einer bevorzugten Ausgestaltung der Erfindung ist vorgesehen, dass in der Destillationskolonne anfallende Schlempe einer die Schlempe in eine Feststofffraktion und eine Dünnsaftfraktion trennenden Trennvorrichtung zuführbar ist, dass der Destillationskolonne zu deren Beheizung ein als Fallfilmverdampfer ausgebildeter, durch Kopfbrüden einer im Produktstrom nachfolgenden, die Alkoholkonzentration erhöhenden Kolonne oder durch Frischdampf beheizter Reboiler zugeordnet ist und zumindest ein Teil der Dünnsaftfraktion in einen Zwangsumlaufkreis durch den Fallfilmverdampfer geführt ist und
dass zumindest ein Teil der in den Zwangsumlaufkreis umlaufenden Dünnsaftfraktion oder Brüden hiervon der Destillationskolonne zu deren Beheizung zuführbar ist. Der als Reboiler der Destillationskolonne benutzte Fallfilmverdampfer kann problemlos in den Energiehaushalt der Destillieranlage integriert werden. Da die Feststofffraktion der Schlempe in der beispielsweise als Dekanter ausgebildeten Trennvorrichtung abgetrennt wird und lediglich die Dünnsaftfraktion durch den Zwangsumlaufkreis zirkuliert, wird die Verschmutzung des an sich verschmutzungsempfindlichen Fallfilmverdampfers weitgehend vermieden. Die abgetrennte Feststofffraktion wird aus dem Prozess entfernt. Zweckmäßigerweise wird der in dem Fallfilmverdampfer erzeugte Brüden direkt in die Destillationskolonne zur Beheizung eingespeist.In a preferred embodiment of the invention it is provided that in the distillation column resulting vinification of a sludge into a solids fraction and a thin juice fraction separating separator is fed to the distillation column to their heating as a falling film evaporator trained by Kopfbrüden one in the product stream subsequent, the alcohol concentration Column or steam-heated reboiler is assigned and at least a portion of the thin juice fraction is passed into a forced circulation loop through the falling film evaporator, and
at least some of the thin juice fraction or vapors circulating in the forced circulation circuit can be supplied to the distillation column for heating thereof. The falling film evaporator used as reboiler of the distillation column can be easily integrated into the energy balance of the distillation unit. Since the solids fraction of the vinasse is separated in the separator, for example, designed as a decanter and only the thin juice fraction circulated through the forced circulation, the pollution of the seepage-sensitive falling film evaporator is largely avoided. The separated solids fraction is removed from the process. Conveniently, the vapor generated in the falling film evaporator is fed directly into the distillation column for heating.

In einer bevorzugten Ausgestaltung wird der den Reboiler der Destillationskolonne bildende Fallfilmverdampfer durch die im Alkoholproduktstrom zwischen der Destillationskolonne und der Rektifikationskolonne angeordneten, die Alkoholkonzentration des Rohalkohols erhöhenden Verstärkungskolonne beheizt. Zwar wird hierdurch ein Teil der zur Beheizung der Verstärkungskolonne aufgewandten Energie rückgewonnen, doch reicht diese Energie unter Umständen für die vollständige Beheizung der Destillationskolonne nicht aus, nachdem die Verstärkungskolonne verglichen mit einer herkömmlichen Rektifikationskolonne auf einem niedrigeren Energieniveau betrieben wird. Im Einzelfall muss deshalb der Energiebedarf der Destillationskolonne anderweitig ergänzt werden.In a preferred embodiment, the falling film evaporator forming the reboiler of the distillation column is heated by the reinforcing column arranged in the alcohol product stream between the distillation column and the rectification column and increasing the alcohol concentration of the crude alcohol. While this recovers some of the energy used to heat the boost column, this energy may not be enough to fully heat the distillation column after the boost column is operated at a lower energy level as compared to a conventional rectification column. In individual cases, therefore, the energy requirement of the distillation column must be supplemented elsewhere.

Für die Ergänzung des Energiebedarfs der Destillationskolonne kann in an sich bekannter Weise ein Zwangsumlaufverdampfer vorgesehen sein, der durch Kopfbrüden der Destillationskolonne beheizt wird. Da der Druck und die Temperatur des Kopfbrüdens der Destillationskolonne für den Betrieb des Zwangsumlaufverdampfers nicht ausreicht, ist es bekannt, den Druck und die Temperatur des Kopfbrüdens mittels eines Verdichters zu erhöhen. Da der Verdichter alkoholhaltigen Brüden verdichtet, muss der Verdichter explosionsgeschützt ausgeführt sein, was den konstruktiven Aufwand beträchtlich erhöht.For supplementing the energy requirement of the distillation column, a forced circulation evaporator can be provided in a manner known per se, which is heated by overhead vapors of the distillation column. Since the pressure and the temperature of the top of the distillation column of the distillation column for the operation of the forced circulation evaporator is not sufficient, it is known to increase the pressure and the temperature of the Kopfbrüdens by means of a compressor. Since the compressor compresses vapors containing alcohol, the compressor must be explosion-proof, which considerably reduces the design effort elevated.

In einer bevorzugten Ausgestaltung ist vorgesehen, dass der Rohalkoholbrüden der Destillationskolonne in einem zur Erzeugung von Wasserdampf genutzten Verdampfer zumindest zu einem Teil kondensierbar ist und der Wasserdampf über einen den Druck oder/und die Temperatur des Wasserdampfs erhöhenden mechanischen Verdichter der Destillationskolonne oder einer weiteren, aus der fermentierten Maische als Rohalkohol abziehenden Destillationskolonne zu deren Beheizung zuführbar ist.In a preferred embodiment, it is provided that the Rohalkoholbrüden the distillation column is at least partially condensable in an evaporator used for the production of steam and the steam over a the pressure and / or the temperature of the water vapor increasing mechanical compressor of the distillation column or another, from the fermented mash can be fed as raw alcohol-withdrawing distillation column to the heating thereof.

Der Verdichter komprimiert damit alkoholfreien Wasserdampf und muss damit nicht explosionsgeschützt ausgeführt sein. Da es sich um einen mechanischen Verdichter handelt, kann er elektrisch angetrieben werden, was sich relativ einfach und kostengünstig realisieren lässt. Der Energiebedarf der Destillationskolonne kann auf diese Weise ergänzt werden, ohne das der Energieinhalt des Kopfbrüdens der Verstärkungskolonne oder einer sonstigen Stufe der Destillieranlage lediglich unter dem Gesichtspunkt der Beheizung der Destillationskolonne erhöht werden müsste.The compressor thus compresses non-alcoholic water vapor and thus does not have to be explosion-proof. Since it is a mechanical compressor, it can be driven electrically, which can be relatively easily and inexpensively. The energy requirement of the distillation column can be supplemented in this way, without the energy content of the overhead vapor of the reinforcing column or any other stage of the distillation would have to be increased only from the viewpoint of heating the distillation column.

Der mittels des mechanischen Verdichters verdichtete Wasserdampf kann der bereits mittels des Reboilers teilbeheizten Destillationskolonne zusätzlich zugeführt werden. Bei einer mehrstufigen, z.B. zweistufigen Destillationskolonne kann eine erste Destillationskolonne mittels des durch Kopfbrüden einer nachfolgenden, die Alkoholkonzentration erhöhenden Kolonne, beispielsweise der Verstärkungskolonne oder Rektifikationskolonne beheizt werden, während die zweite Destillationskolonne durch den verdichteten Wasserdampf des mechanischen Verdichters beheizt wird. Den beiden Destillationskolonnen wird die Maische parallel zugeführt, wobei jedoch die zweite Destillationskolonne bevorzugt bei einer tieferen Kopftemperatur und niedrigerem Druck betrieben wird als die erste Destillationskolonne.The compressed by means of the mechanical compressor water vapor can be additionally supplied to the already partially heated by the reboiler distillation column. In a multistage, eg two-stage distillation column, a first distillation column can be heated by head vapor of a subsequent column increasing the alcohol concentration, for example the amplification column or rectification column, while the second distillation column is heated by the compressed water vapor of the mechanical compressor. The two distillation columns, the mash is fed in parallel, but the second distillation column is preferably operated at a lower head temperature and lower pressure than the first distillation column.

Bevorzugt handelt es sich bei dem den Wasserdampf erzeugenden Verdampfer um einen Fallfilmverdampfer, um auch hier die im Fall des Fallfilmverdampfers niedrige Temperaturdifferenz zwischen Heiztemperatur und Verdampfungstemperatur energetisch nutzen zu können. Der Fallfilmverdampfer ist zweckmäßigerweise für die Erzeugung des Wasserdampfs in einem Zirkulationskreis für Frischwasser oder Schlempe oder Schlempebrüden angeordnet. Die Erzeugung des Wasserdampfs aus Schlempe oder Schlempebrüden hat den Vorteil, dass der Wasserdampf hinreichende Temperatur hat, da die Schlempe aus dem beheizten Fußbereich der Destillationskolonne abgezogen wird. Wird Frischwasser genutzt, so muss dieses vorgewärmt werden. Allerdings wird bei Nutzung von Frischwasser vermieden, dass sich in der Schlempe enthaltene Komponenten durch Crackreaktionen in leichtflüchtige Stoffe verwandeln, die in den Rohalkohol gelangen können. Die Nutzung von Frischwasser minimiert Denaturierungsreaktionen und Ablagerungen in dem Fallfilmverdampfer. Der mechanische Verdichter ist dennoch bevorzugt über einen den Wasserdampf abtrennenden Abscheider, insbesondere einem Entspannungsabscheider an den Zirkulationskreis angeschlossen.The vapor-generating evaporator is preferably a falling-film evaporator in order to be able to use the low temperature difference between heating temperature and evaporation temperature in the case of the falling-film evaporator. The falling-film evaporator is expediently arranged for the generation of the steam in a circulation circuit for fresh water or stillage or vapors. The generation of steam from vinasse or vinasse has the advantage that the steam has sufficient temperature, since the vinasse is withdrawn from the heated foot region of the distillation column. If fresh water is used, it must be preheated. However, the use of fresh water avoids that components contained in the vinasse are transformed by cracking reactions in volatile substances that can reach the raw alcohol. The use of fresh water minimizes denaturation reactions and deposits in the falling film evaporator. The mechanical compressor is nevertheless preferably connected to the circulation circuit via a separator separating the steam, in particular a flash separator.

Der mechanische Verdichter kann als Kompressor aufgebaut sein oder als Schaufelradverdichter. Es versteht sich, dass der Verdichter auch mehrere seriell verbundene mechanische Verdichterstufen umfassen kann.The mechanical compressor may be constructed as a compressor or as a paddle wheel compressor. It is understood that the compressor may also include a plurality of serially connected mechanical compressor stages.

Im Folgenden wird die Erfindung anhand einer Zeichnung näher erläutert. Die Figur der Zeichnung zeigt ein schematisches Schaltbild einer Ethylalkohol aus fermentierter Maische erzeugenden Destillieranlage.In the following the invention will be explained in more detail with reference to a drawing. The figure of the drawing shows a schematic diagram of an ethyl alcohol from fermented mash-producing distillation plant.

Der für die Erzeugung von Ethylalkohol als Kraftstoff für Brennkraftmaschinen oder für Industriezwecke geeigneten Destillieranlage wird aus einer Vorstufe 1 des Alkoholherstellungsprozesses fermentierte, d.h. vergorene und damit ethylalkoholhaltige Maische eines nachwachsenden Agrarrohstoffs mit relativ hohem Proteinanteil, wie z.B. Roggen, Weizen, Gerste usw. zugeführt. Die Maische wird in einem Vorwärmer 3 auf die Destillationstemperatur einer Destillationskolonne 5 erwärmt und der Destillationskolonne 5 über eine Leitung 7 zugeführt. Der Kopfbereich, der vielfach auch als Maischekolonne bezeichneten Destillationskolonne 5 ist bei 11 angedeutet, ihr Fußbereich bei 13.The distilling plant suitable for the production of ethyl alcohol as a fuel for internal combustion engines or for industrial purposes is fermented from a precursor 1 of the alcohol production process, ie fermented and thus ethyl alcohol-containing mash of a relatively high-protein agricultural raw material, such as rye, wheat, Barley, etc. supplied. The mash is heated in a preheater 3 to the distillation temperature of a distillation column 5 and fed to the distillation column 5 via a line 7. The head region, often also referred to as mashing column distillation column 5 is indicated at 11, her foot at 13.

Die aus dem Kopfbereich 11 der Destillationskolonne 5 als Alkoholbrüden abgezogene Rohalkohol wird in einer hier mehrstufigen und zugleich der Energierückgewinnung der in dem Rohalkohol enthaltenen Wärmeenergie genutzten Kondensatoranordnung 15 kondensiert und in flüssiger Form mittels einer Förderpumpe 17 über einen den Rohalkohol auf die Rektifikationstemperatur einer Verstärkungskolonne 19 erwärmenden Vorwärmer 21 bei 23 als Zulauf zugeführt. Die Verstärkungskolonne 19 erhöht den Alkoholgehalt des Rohalkohols der Destillationskolonne im Kopf bereits auf etwa 94 Vol%; das verbleibende Ethanol im Sumpf wird in der Rektifikationskolonne 33 vom Lutterwasser getrennt.The crude alcohol withdrawn from the head region 11 of the distillation column 5 as alcohol vapors is condensed in a multistage and at the same time energy recovery of the thermal energy contained in the crude alcohol and condensed in liquid form by means of a feed pump 17 via a raw alcohol to the rectification temperature of a booster column 19 Preheater 21 fed at 23 as an inlet. The reinforcing column 19 already increases the alcohol content of the crude alcohol of the distillation column in the head to about 94% by volume; the remaining ethanol in the bottom is separated from the lutter water in the rectification column 33.

Der aus dem Kopfbereich 25 der Verstärkungskolonne 19 abgezogene, rektifizierte Alkoholbrüden wird, wie nachfolgend noch näher erläutert wird, in einem die Destillationskolonne 5 beheizenden, als Kopfkondensator der Verstärkungskolonne 19 ausgenutzten Reboiler 27 kondensiert und mittels einer Förderpumpe 29 sowohl dem Kopfbereich 25 der Verstärkungskolonne 19 als auch dem Kopfbereich 31 einer der Verstärkungskolonne 19 nachgeschalteten Rektifikationskolonne 33 als Rücklauf zugeführt. Als Zulauf der Rektifikationskolonne 33 dient Ethanol-Wasser-Gemisch, das über einen Zwangsumlaufkreis 35 mittels einer Förderpumpe 37 aus dem Fußbereich 39 der Verstärkungskolonne 19 abgezogen und über eine Leitung 41 der Rektifikationskolonne 33 zugeführt wird.The rectified alcohol vapor withdrawn from the head region 25 of the amplification column 19 is, as will be explained in more detail below, condensed in a reboiler 27 which heats the distillation column 5 and used as a top condenser of the amplification column 19 and by means of a feed pump 29 both to the head region 25 of the amplification column 19 also fed to the head region 31 of a rectification column 33 connected downstream of the amplification column 19 as reflux. The feed of the rectification column 33 is ethanol-water mixture, which is withdrawn via a forced circulation circuit 35 by means of a feed pump 37 from the foot region 39 of the reinforcing column 19 and fed via a line 41 of the rectification column 33.

Der in der Rektifikationskolonne 33 weiter aufkonzentrierte Ethylalkohol wird in einer Molekularsiebanordnung 43 dehydriert und steht als rektifizierter und dehydrierter Ethylalkohol bei 45 als Endprodukt zur Verfügung.The further concentrated in the rectification column 33 ethyl alcohol is dehydrated in a molecular sieve assembly 43 and is available as a rectified and dehydrated ethyl alcohol at 45 as an end product.

Der Energiebedarf der Destillieranlage wird in erster Linie durch den Energiebedarf der Aufkonzentrierung und weniger durch das Abziehen des Rohalkohols aus der Maische bestimmt. Die Rektifizierung erfolgt in zwei Stufen, d.h. in der Verstärkungskolonne 19 und der Rektifikationskolonne 33. Da der Rückfluss der Rektifikationskolonne 33 dem Kopfprodukt der Verstärkungskolonne 19 und der Zufluss der Rektifikationskolonne 33 dem Fußbereich 39 der Verstärkungskolonne 19 entnommen wird, ist die Temperaturdifferenz des Fußbereichs 39 zum Kopfbereich 25 der Verstärkungskolonne 19 vergleichsweise gering, so dass sich die Verstärkungskolonne 19 selbst dann gut in den Wärmehaushalt der Destillieranlage integrieren lässt, wenn die Rektifikationskolonne 33 lediglich bei einer Kopftemperatur zwischen 85 und 110°C betrieben wird. Wesentlich für die Verringerung des Energiebedarfs der Destillieranlage ist, dass die Rektifikationskolonne 33 den Alkohol lediglich auf etwa 94 Vol% aufkonzentriert, bevor der rektifizierte Alkohol der Molekularsiebanordnung 43 zur Dehydrierung zugeführt wird. Zugleich wird die Destillationstemperatur der Destillationskolonne 5 auf eine Temperatur von weniger als 85°C begrenzt, so dass der Destillierprozess auf einem niedrigeren Energieniveau als bisher durchgeführt wird.The energy requirement of the distillation plant is determined primarily by the energy requirement of the concentration and less by the removal of raw alcohol from the mash. The rectification takes place in two stages, i. In the booster column 19 and the rectification column 33. Since the reflux of the rectification column 33 is taken from the top product of the booster column 19 and the inflow of the rectification column 33 to the bottom portion 39 of the booster column 19, the temperature difference of the base portion 39 to the top portion 25 of the booster column 19 is comparatively low. so that the reinforcing column 19 can be well integrated into the heat balance of the distillation still even if the rectification column 33 is operated only at a head temperature between 85 and 110 ° C. It is essential for the reduction of the energy requirement of the distillation plant that the rectification column 33 only concentrates the alcohol to about 94% by volume before the rectified alcohol is fed to the molecular sieve arrangement 43 for dehydrogenation. At the same time the distillation temperature of the distillation column 5 is limited to a temperature of less than 85 ° C, so that the distillation process is carried out at a lower energy level than before.

Der durch Kopfbrüden der Verstärkungskolonne 19 beheizte und den Kopfbrüden kondensierende Reboiler 27 ist als Fallfilmverdampfer ausgebildet und beheizt den Fußbereich 13 der Destillationskolonne 5. Die in der Destillationskolonne 5 anfallende, alkoholfreie Schlempe wird über einen Fußbereichsauslass 49 einem Dekanter 51 zugeführt, der die Schlempe in eine bei 53 aus dem Prozess entfernte Feststofffraktion und eine über eine Leitung 54 stromabwärts des Reboilers 27 jedoch vor einer Förderpumpe 56 in den Zwangsumlaufkreis 47 eingeleitete Dünnsaftfraktion aufteilt. In den Zwangsumlaufkreis 47 zirkuliert damit anders als bei herkömmlichen Reboilern auf der Basis eines Zwangsumlaufverdampfers nicht Schlempe, sondern deren von Feststoffen weitestgehend befreite Dünnsaftfraktion. Ein Teil der in dem Fallfilmverdampfer 27 erwärmten Dünnsaftfraktion der Schlempe oder daraus gewonnener Brüden wird bei 58 direkt in den Fußbereich 13 der Destillationskolonne 5 zu deren Beheizung zurückgeführt. Der Vorteil des Fallfilmverdampfers 27, dass die Temperatur des an seinem den Kopfbrüden der Verstärkungskolonne 19 aufnehmenden Anschluss zugeführten Kopfbrüdens nur wenig größer, beispielsweise 5°C höher als die Siedetemperatur des zu verdampfenden Produkts, hier der Dünnsaftfraktion, sein muss, erleichtert die Einbindung der Anlage in die Energiebilanz der Destillieranlage. Die zum Beheizen der Destillationskolonne 5 erforderliche Energiemenge kann damit auf einem niedrigeren Temperaturniveau als bisher bereitgestellt werden.The reboiler 27 which is heated by head vapor of the amplification column 19 and condenses the head vapor is designed as a falling film evaporator and heats the foot region 13 of the distillation column 5. The non-alcoholic stillage obtained in the distillation column 5 is fed via a foot region outlet 49 to a decanter 51 which separates the vinasse into a at 53 removed from the process solids fraction and a via a line 54 downstream of the reboiler 27 but before a feed pump 56 into the forced circulation 47 split thin juice fraction divided. Thus, unlike conventional reboilers based on a forced circulation evaporator, the forced circulation circuit 47 does not circulate the still, but rather the thin juice fraction which is largely freed of solids. Some of the thin juice fraction of the vinasse or vapors recovered therefrom heated in the falling film evaporator 27 becomes directly in the foot region at 58 13 of the distillation column 5 returned to the heating. The advantage of the falling-film evaporator 27 that the temperature of the head vapor supplied at its head receiving head of the booster column 19 is only slightly greater, for example 5 ° C. higher than the boiling point of the product to be vaporized, here the thin juice fraction, facilitates the integration of the system into the energy balance of the distillation plant. The amount of energy required to heat the distillation column 5 can thus be provided at a lower temperature level than heretofore.

Bei dem dargestellten Ausführungsbeispiel wird die Schlempe an einer zuunterst im Fußbereich 13 liegenden Stelle abgezogen. Es versteht sich, dass die Schlempe auch an einer darüber liegenden Stelle, beispielsweise im Bereich des untersten Bodens der Destillationskolonne 5 abgezogen werden kann, so dass der die Dünnsaftfraktion führende Zwangsumlaufkreis 47 ggf. auch direkt durch den Fußbereich 13 verlaufen kann.In the illustrated embodiment, the vinasse is withdrawn at a lowermost located in the foot area 13 point. It is understood that the vinasse can also be withdrawn at an overlying location, for example in the region of the lowest bottom of the distillation column 5, so that the forced circulation circuit 47 carrying the thin juice fraction can if necessary also run directly through the foot region 13.

Die den Rohalkoholbrüden aus dem Kopfbereich 11 der Destillationskolonne 5 kondensierende Kondensatoranordnung 15 umfasst als erste Stufe einen Fallfilmverdampfer 55 zur Erzeugung von Niederdruck-Wasserdampf, der über einen Entspannungs-Schwerkraftabscheider 57 an einen mechanischen Verdichter 59 abgegeben wird. Der mechanische Verdichter 59 erhöht den Druck und die Temperatur des Wasserdampfs und bläst den verdichteten Wasserdampf unmittelbar in den Fußbereich 13 zur zusätzlichen Beheizung der Destillationskolonne 5 ein. Auf diese Weise wird ein Teil der Kondensationswärme des Rohalkohol-Kopfbrüdens der Destillationskolonne 5 für die Beheizung der Destillationskolonne zurückgewonnen. Da der mechanische Verdichter 59 anders als bei herkömmlichen Brüdenverdichtern nicht Alkoholbrüden verdichtet, sondern Wasserdampf, muss der Verdichter 59 nicht explosionsgeschützt ausgeführt sein.The condenser assembly 15 condensing the crude alcohol vapors from the head region 11 of the distillation column 5 comprises, as a first stage, a falling-film evaporator 55 for generating low-pressure steam which is discharged to a mechanical compressor 59 via an expansion gravity separator 57. The mechanical compressor 59 increases the pressure and the temperature of the water vapor and blows the compressed steam directly into the foot region 13 for additional heating of the distillation column 5. In this way, a portion of the heat of condensation of the crude alcohol overheads of the distillation column 5 is recovered for the heating of the distillation column. Since the mechanical compressor 59, unlike conventional vapor compressors, does not compress alcohol vapor but water vapor, the compressor 59 does not have to be explosion-proof.

Der Fallfilmverdampfer 55 ist in einer mit einer Pumpe 61 versehenen Zwangsumlaufkreis 63 angeordnet, und verdampft in dem Zwangsumlaufkreis zirkulierendes Frischwasser, das bei 65 aus einer nicht dargestellten Quelle in vorgewärmter Form zugeführt wird. Aus dem Zwangsumlaufkreis 47 stromab der Pumpe 56 ablaufende Dünnsaftfraktion bzw. Dünnschlempe wird über den Abscheider 57 dem Zwangsumlaufkreis 63 des Fallfilmverdampfers 55 ergänzend zur Frischwasserzufuhr zugeführt und verlässt den Zwangsumlaufkreis 63 und damit den Prozess bei 67.The falling-film evaporator 55 is disposed in a forced circulation circuit 63 provided with a pump 61, and evaporates in the forced circulation circuit circulating fresh water which is supplied at 65 from a source, not shown, in preheated form. From the forced circulation circuit 47 downstream of the pump 56 running thin juice fraction or Dünnschlempe is supplied via the separator 57 to the forced circulation circuit 63 of the falling film evaporator 55 in addition to the fresh water supply and leaves the forced circulation circuit 63 and thus the process at 67.

Der Niederdruck-Wasserdampf hat eingangsseitig des Verdichters 59 einen Druck von beispielsweise etwa 200 bis 250 mbar und wird von dem Verdichter 59 auf einen Ausgangsdruck zwischen 500 und 600 mbar bei einer Temperatur zwischen 70 und 90°C angehoben. Der mechanische Verdichter kann als einstufiger oder auch als mehrstufiger Verdichter ausgebildet sein. Geeignet sind rotierende Kompressoren, aber auch Schaufelradverdichter bzw. Ventillatoren. Da der Verdichter 59 elektromotorisch angetrieben wird, lässt sich die Antriebsenergie einfacher zur Verfügung stellen, als dies beispielsweise bei einem Dampfstrahlverdichter möglich ist.The low-pressure steam has on the input side of the compressor 59, a pressure of for example about 200 to 250 mbar and is raised by the compressor 59 to an outlet pressure between 500 and 600 mbar at a temperature between 70 and 90 ° C. The mechanical compressor can be designed as a single-stage or as a multi-stage compressor. Suitable are rotating compressors, but also bucket wheel compressors or Ventillatoren. Since the compressor 59 is driven by an electric motor, the drive energy can be made available more simply than is possible, for example, with a steam jet compressor.

Die Destillationskolonne 5 arbeitet zweckmäßigerweise bei einer Kopftemperatur zwischen 55 und 75°C und einem Kopfdruck zwischen 300 und 500 mbar. Im Prinzip könnte anstelle des Fallfilmverdampfers 55 auch ein anderer Verdampfertyp eingesetzt werden. Vorteil des Fallfilmverdampfers ist jedoch seine geringe Temperaturdifferenz von beispielsweise 5°C zwischen der Eingangstemperatur des zumindest teilweise zu kondensierenden Rohalkoholbrüdens der Destillationskolonne 5 und der Ausgangstemperatur des Niederdruck-Wasserdampfs. Die Verdichterleistung des Verdichters 59 kann auf dieser Weise verringert werden.The distillation column 5 expediently operates at a head temperature between 55 and 75 ° C and a top pressure between 300 and 500 mbar. In principle, instead of the falling film evaporator 55, another type of evaporator could also be used. Advantage of the falling film evaporator, however, is its low temperature difference of, for example, 5 ° C between the inlet temperature of the at least partially to be condensed Rohalkoholbrüdens the distillation column 5 and the outlet temperature of the low-pressure steam. The compressor capacity of the compressor 59 can be reduced in this way.

Nicht näher dargestellt ist eine Variante, bei welcher der in vorstehend erläuterter Weise von dem Fallfilmverdampfer 55 mit der Kondensationswärme der Destillationskolonne 5 erzeugte und durch den Verdichter 59 verdichtete Wasserdampf nicht der Destillationskolonne 5 zur Beheizung zugeführt wird, sondern einer weiteren Destillationskolonne, deren Rohalkoholbrüden dann den Vorwärmer 3 betreibt. Da diese weitere Destillationskolonne bei einer niedrigeren Destillationstemperatur betrieben wird als die Destillationskolonne 5, kann die für den Betrieb des mechanischen Verdichters 59 aufzuwendende elektrische Energie weiter verringert werden. Die beiden Destillationskolonnen werden, was die Zuführung der Maische anbelangt, parallel und was den Energiehaushalt anbelangt, in Serie betrieben.Not shown in detail is a variant in which the manner described above by the falling film evaporator 55 with the heat of condensation of the distillation column 5 and compressed by the compressor 59 steam is not supplied to the distillation column 5 for heating, but a further distillation column, the Rohalkoholbrüden then the Preheater 3 operates. Because these more Distillation column is operated at a lower distillation temperature than the distillation column 5, the expended for the operation of the mechanical compressor 59 electrical energy can be further reduced. The two distillation columns are, as far as the supply of mash, parallel and as far as the energy budget, operated in series.

Im dargestellten Ausführungsbeispiel wird dem Zwangsumlaufkreis 63 Frischwasser zugeführt, was die Gefahr von Denaturierungsreaktionen und Nebenkomponentenbildung mindert. Es versteht sich, dass in den Zwangsumlaufkreis 63 auch ausschließlich mit Dünnsaftfraktion bzw. Dünnschlempe gearbeitet werden kann.In the illustrated embodiment, the forced circulation circuit 63 fresh water is supplied, which reduces the risk of Denaturierungsreaktionen and secondary component formation. It is understood that it is also possible to work exclusively with thin juice fraction or thin still in the forced circulation circuit 63.

Da der Rohalkohol-Kopfbrüden der Destillationskolonne 5 in dem Fallfilmverdampfer 55 nicht vollständig kondensiert, wird der nicht kondensierte Brüdenanteil bei 69 dem die zweite Stufe der Kondensationsanordnung 15 bildenden Vorwärmer 3 für die Vorwärmung der Maische zugeführt. Der Ausgangsbrüden des Vorwärmers 3 wird schließlich einem Hauptkondensator 71 zugeführt, der die dritte Stufe der Kondensationsanordnung 15 bildet und den Rohalkohol als flüssiges Kondensat über die Förderpumpe 17 zur Weiterleitung an die Verstärkungskolonne 19 abgibt. Der Hauptkondensator 71 ist an eine Kühlwasserquelle 73 angeschlossen und ist überdies mit einer Vakuumpumpe 75 verbunden, über die der Unterdruck in der Destillieranlage eingestellt wird.Since the crude alcohol overhead vapor of the distillation column 5 in the falling film evaporator 55 is not completely condensed, the uncondensed vapor fraction at 69 is fed to the preheater 3 for preheating the mash, forming the second stage of the condensation assembly 15. The Ausgangsbrüden of the preheater 3 is finally fed to a main capacitor 71, which forms the third stage of the condensation assembly 15 and the raw alcohol as liquid condensate via the feed pump 17 emits for forwarding to the reinforcing column 19. The main condenser 71 is connected to a cooling water source 73 and is also connected to a vacuum pump 75, via which the negative pressure in the distillation unit is set.

Im dargestellten Ausführungsbeispiel wird die Maische der Destillationskolonne 5 nahe ihres Kopfbereichs 11 zugeführt, also auf einen von der Verstärkungskolonne 19 gesonderten Verstärkungsbereich verzichtet. Dementsprechend hat der den Hauptkondensator 71 verlassende Rohalkohol eine Konzentration von lediglich 40 bis 60 Vol%. Der Energiebedarf der Destillationskolonne 5 ist damit vergleichsweise gering. Die Aufkonzentration des Rohalkohols erfolgt in der Verstärkungskolonne 19 und nachfolgend der Rektifikationskolonne 33. Da die Rektifikation auf zwei Stufen verteilt ist, kann auch hier energetisch günstig gearbeitet werden. Es versteht sich jedoch, dass auch die Destillationskolonne 5 in gewissem Umfang zusätzliche Böden zur Aufkonzentration umfassen kann.In the illustrated embodiment, the mash of the distillation column 5 is supplied near its top portion 11, so dispensed with a separate from the gain column 19 gain range. Accordingly, the raw alcohol leaving the main condenser 71 has a concentration of only 40 to 60% by volume. The energy requirement of the distillation column 5 is thus comparatively low. The concentration of the crude alcohol takes place in the reinforcing column 19 and subsequently the rectification column 33. Since the rectification is distributed in two stages, can be worked here energetically favorable. It is understood, however, that also the distillation column 5 may to some extent comprise additional soils for concentration.

Die Verstärkungskolonne 19 wird in erster Linie durch einen als Fallfilmverdampfer ausgebildeten Reboiler 77 beheizt, der zugleich den Kopfkondensator der Rektifikationskolonne 33 bildet. Der Reboiler 77 ist an den durch den Fußbereich 39 der Verstärkungskolonne 19 führenden Zwangsumlaufkreis 35 angeschlossen.The reinforcing column 19 is heated primarily by a reboiler 77 designed as a falling-film evaporator, which at the same time forms the top condenser of the rectification column 33. The reboiler 77 is connected to the forced circulation circuit 35 leading through the foot region 39 of the reinforcing column 19.

Die Rektifikationskolonne 33 wird in ähnlicher Weise in erster Linie über einen als Fallfilmverdampfer ausgebildeten Reboiler 79 beheizt, der an einen durch den Fußbereich 81 der Rektifikationskolonne 33 geführten Zwangsumlaufkreis 83 angeschlossen ist. Eine Förderpumpe des Zwangsumlaufkreises 83 ist bei 85 dargestellt. Beheizt wird der Reboiler 79 durch Frischdampf, der ihm aus einer Frischdampfquelle 87 über eine Leitung 89 zugeführt wird. In dem Zwangsumlaufkreis 83 zirkulierendes Lutterwasser aus dem Fußbereich 81 wird stromab der Pumpe 85 über eine Leitung 91 abgezogen und, nachdem es in dem Vorwärmer 21 zur Vorerwärmung des der Verstärkungskolonne 19 zugeführten, flüssigen Rohalkohols ausgenutzt wurde, bei 93 aus dem Prozess entfernt.The rectification column 33 is heated in a similar manner primarily via a reboiler 79 designed as a falling-film evaporator, which is connected to a forced circulation circuit 83 guided through the foot region 81 of the rectification column 33. A feed pump of the forced circulation circuit 83 is shown at 85. The reboiler 79 is heated by live steam, which is supplied to it from a live steam source 87 via a line 89. Lutter water circulating in the forced circulation circuit 83 from the foot region 81 is withdrawn downstream of the pump 85 via a line 91 and removed from the process at 93 after it has been utilized in the preheater 21 to preheat the crude liquid alcohol fed to the boost column 19.

Während die Verstärkungskolonne 19 etwa 30 Böden hat, umfasst die Rektifikationskolonne 33 etwa 50 Böden und liefert den rektifizierten Alkohol bei einem Druck von etwa 1,5 bis 6 bar, beispielsweise 2 bar, an einem Seitenabzug 95 in Dampfform bei einer Alkoholkonzentration von etwa 94 Vol%. Der dampfförmige, rektifizierte Alkohol wird einem gleichfalls aus der Frischdampfquelle 87 beheizten Überhitzer 97 zugeführt, der den überhitzten Alkoholdampf bei 99 der Molekularsiebanordnung 43 zur Dehydrierung zuführt.While the boost column 19 has about 30 trays, the rectification column 33 comprises about 50 trays and provides the rectified alcohol at a pressure of about 1.5 to 6 bar, for example 2 bar, on a side draw 95 in vapor form at an alcohol concentration of about 94 vol %. The vaporous, rectified alcohol is fed to a likewise heated from the live steam source 87 superheater 97, which supplies the superheated alcohol vapor at 99 of the molecular sieve assembly 43 for dehydration.

Die Molekularsiebanordnung 43 weist in an sich bekannter Weise mehrere Molekularsiebe, hier drei Molekularsiebe 101, 103 und 105 auf, die in zyklischer Vertauschung jeweils in einem Trocknungsmodus und einem Regenerationsmodus betrieben werden. Im dargestellten Ausführungsbeispiel arbeitet jeweils ein Molekularsieb, hier das Molekularsieb 101 im Trocknungsmodus, während die beiden anderen Molekularsiebe 103, 105 in ihren Regenerationsmodus geschaltet sind.The molecular sieve arrangement 43 has, in a manner known per se, a plurality of molecular sieves, in this case three molecular sieves 101, 103 and 105, which in FIG cyclic permutation in each case in a drying mode and a regeneration mode. In the illustrated embodiment, in each case a molecular sieve, in this case the molecular sieve 101, operates in the drying mode, while the other two molecular sieves 103, 105 are switched into their regeneration mode.

Im Trocknungsmodus wird der dampfförmige, überhitzte Alkohol unter erhöhtem Druck dem aktuell im Trocknungsmodus arbeitenden Molekularsieb, hier dem Molekularsieb 101 zugeführt, das den dehydrierten Alkohol an eine Sammelleitung 107 abgibt, an die die Molekularsiebe 101, 103, 105 mit ihren Ausgängen für dehydrierten Alkohol gemeinsam angeschlossen sind.In the drying mode, the superheated vaporous alcohol is fed to the molecular sieve currently operating in the drying mode, here the molecular sieve 101, which delivers the dehydrated alcohol to a manifold 107 to which the molecular sieves 101, 103, 105 share their dehydrated alcohol exits are connected.

Die aktuell im Regenerationsmodus betriebenen Molekularsiebe 103, 105 sind für den Betrieb im Regenerationsmodus über einen Kondensator 109 an eine Vakuumquelle 111 angeschlossen, die den Molekularsieben 103, 105 über die Sammelleitung 107 zugeführten dehydrierten Alkohol in Rückwärtsrichtung durch die zu regenerierenden Molekularsiebe 103, 105 und durch den Kondensator 109 saugt. Der Kondensator 109 wird aus der Kühlwasserquelle 73 mit Kühlwasser versorgt und kondensiert das bei der Regeneration in den Molekularsieben 103, 105 sich erneut befeuchtende Alkohol-Wasserdampf-Gemisch. Eine Pumpe 113 fördert das in einem Sammelbehälter 115 sich sammelnde Alkohol-Wasser-Gemisch in dem Prozess zurück.The regeneration mode molecular sieves 103, 105 are connected to a vacuum source 111 via a condenser 109 for regeneration mode operation, and the dehydrogenated alcohol fed back to the molecular sieves 103, 105 through the regenerated molecular sieves 103, 105 and through the dehydrated alcohol fed through the manifold 107 sucks the capacitor 109. The condenser 109 is supplied with cooling water from the cooling water source 73 and condenses the alcohol-water vapor mixture rehydrated in the molecular sieves 103, 105 during regeneration. A pump 113 conveys the alcohol-water mixture collecting in a collecting tank 115 in the process.

Es versteht sich, dass die Anzahl der Molekularsiebe von dem dargestellten Ausführungsbeispiel abweichen kann. Für einen kontinuierlichen Betrieb sind mindestens zwei Molekularsiebe erforderlich, die wechselweise im Trocknungsmodus und Regenerierungsmodus arbeiten. Da der Regenerierungsmodus länger dauern kann als die für die Dehydrierung nutzbare Trocknungszyklusdauer, ist die Anzahl der im Regenerierungsmodus betriebenen Molekularsiebe zweckmäßigerweise größer als die Zahl der im Trocknungsmodus betriebenen Molekularsiebe. Die für die zyklische Vertauschung und Umschaltung der Molekularsiebe erforderlichen steuerbaren Verbindungsleitungen sind bei 117 angedeutet.It is understood that the number of molecular sieves may differ from the illustrated embodiment. For continuous operation, at least two molecular sieves are required, operating alternately in the drying mode and the regeneration mode. Since the regeneration mode may last longer than the dehydration usable drying cycle time, the number of molecular sieves operated in the regeneration mode is desirably greater than the number of molecular sieves operated in the drying mode. The for the cyclical Exchange and switching of the molecular sieves required controllable connection lines are indicated at 117.

Das im Regenerationsmodus anfallende Alkohol-Wasser-Gemisch wird erneut der Rektifikation zugeführt. Da das Gemisch bei der Kondensation im Kondensator 109 auf eine Temperatur von etwa 40°C abgekühlt wurde, wird es in einem Vorwärmer 119 vorgewärmt und über eine Leitung 121 einem Zwangsumlaufkreis 123 eines hier als Fallfilmverdampfer ausgebildeten Verdampfers 125 zugeführt. Der Verdampfer 125 wird gleichfalls mit Frischdampf aus der Frischdampfquelle 87 beheizt und gibt das auf Rektifikationstemperatur erwärmte Gemisch bei 127 als Zulauf an die Rektifikationskolonne 33 ab. Eine Förderpumpe des Zwangsumlaufkreises 123 ist bei 129 dargestellt.The resulting in the regeneration mode alcohol-water mixture is fed again to the rectification. Since the mixture was cooled in the condensation in the condenser 109 to a temperature of about 40 ° C, it is preheated in a preheater 119 and fed via a line 121 to a forced circulation circuit 123 of a here designed as a falling film evaporator evaporator 125. The evaporator 125 is likewise heated with live steam from the live steam source 87 and releases the mixture heated to the rectification temperature at 127 as feed to the rectification column 33. A feed pump of the forced circulation circuit 123 is shown at 129.

In dem durch Frischdampf aus der Frischdampfquelle 87 beheizten Überhitzer 97 bzw. dem Fallfilmverdampfer 79 sowie dem Verdampfer 125 anfallendes Heizdampfkondensat wird über Leitungen 131, 133 und 135 bei 137 aus dem Prozess abgezogen.In the superheater 97 heated by live steam from the live steam source 87 or the falling film evaporator 79 and the evaporator 125 resulting heating steam condensate is withdrawn via lines 131, 133 and 135 at 137 from the process.

Der in der Molekularsiebanordnung 43 dehydrierte Alkohol heizt einen weiteren, als Fallfilmverdampfer ausgebildeten Reboiler 139 der Verstärkungskolonne 19, der parallel zu dem Reboiler 77 an den Zwangsumlaufkreis 35 angeschlossen ist. Der dehydrierte Alkohol wird dem Reboiler 139 aus der Sammelleitung 107 zugeführt und über eine Förderpumpe 141 dem Vorwärmer 119 zur Vorerwärmung des im Regenerationsmodus der Molekularsiebanordnung 43 anfallenden Alkohol-Wasser-Gemisches zugeführt wird, um letztendlich bei 45 als Endprodukt abgezogen zu werden.The alcohol dehydrogenated in the molecular sieve arrangement 43 heats a further reboiler 139, formed as a falling-film evaporator, of the booster column 19, which is connected in parallel to the reboiler 77 to the forced circulation circuit 35. The dehydrated alcohol is supplied to the reboiler 139 from the manifold 107 and fed via a feed pump 141 to the preheater 119 for preheating the alcohol-water mixture obtained in the regeneration mode of the molecular sieve assembly 43, to finally be withdrawn at 45 as the final product.

Der Reboiler 27 der Destillationskolonne 5 bildet zugleich den Kopfkondensator der Verstärkungskolonne 19, während der Reboiler 77 der Verstärkungskolonne 19 zugleich den Kopfkondensator der Rektifikationskolonne 33 bildet. Das in den Reboilern 27 und 77 bei 143 bzw. 145 anfallende Alkoholkondensat wird, gefördert von der Förderpumpe 29 bei 147 der Verstärkungskolonne und bei 149 der Rektifikationskolonne im Kopfbereich als Rückfluss zugeführt. Im Rektifikationsprozess anfallendes Fuselöl wird bei 151 aus der Verstärkungskolonne und bei 153 aus der Rektifikationskolonne abgezogen und bei 155 aus dem Prozess entfernt.The reboiler 27 of the distillation column 5 also forms the top condenser of the reinforcing column 19, while the reboiler 77 of the reinforcing column 19 at the same time forms the top condenser of the rectification column 33. The alcohol condensate obtained in the reboilers 27 and 77 at 143 and 145, respectively, is conveyed by the feed pump 29 147 of the reinforcing column and fed at 149 of the rectification column in the head region as reflux. Fusel oil accumulating in the rectification process is withdrawn at 151 from the boost column and at 153 from the rectification column and removed from the process at 155.

Die vorstehend erläuterte Destillieranlage erlaubt es in einem Niedertemperaturverfahren Ethylalkohol aus Weizen, Roggen usw. zu destillieren. Während herkömmliche Anlagen etwa 2 kg Heizdampf pro Liter reinen Alkohols, entsprechend etwa 4000 kJ pro Liter reinen Alkohols benötigen, erfordert die erfindungsgemäße Destillieranlage lediglich etwa 2300 kJ pro Liter reinen Alkohols zuzüglich etwa 54 W pro Liter reinen Alkohols an elektrischer Energie für die Brüdenverdichtung.The above-described distillation plant allows to distill ethyl alcohol from wheat, rye, etc. in a low-temperature process. While conventional plants require about 2 kg of heating steam per liter of pure alcohol, corresponding to about 4000 kJ per liter of pure alcohol, the distilling plant according to the invention requires only about 2300 kJ per liter of pure alcohol plus about 54 W per liter of pure alcohol in electrical energy for the vapor compression.

Claims (21)

  1. System for distilling alcohol, in particular ethyl alcohol from fermented mash, comprising at least one distillation column (5) which draws off raw alcohol from the fermented mash and has a reboiler (27), and a rectification column (33) which is connected downstream from the distillation column (5) and increases the alcohol concentration, an intensifying column (19) which concentrates the raw alcohol of the distillation column being connected downstream of the at least one distillation column (5), the top vapour condensate of which intensifying column can be supplied to the rectification column (33) as a top-side return flow, and from the foot region (39) of which intensifying column an alcohol-water mixture can be supplied to the rectification column (33) as a flow to be concentrated, the top vapour from the intensifying column (19) being used to heat the distillation column (5), the reboiler (27) of the distillation column (5), which reboiler is heated by means of the top vapour, simultaneously forming the condenser of the intensifying column (19), characterised in that a molecular sieve assembly (43) for dehydrogenating the rectified alcohol is connected downstream of the rectification column (33).
  2. System according to claim 1, characterised in that the system is designed such that the distillation column (5) draws off the raw alcohol at a distillation temperature of less than 85°C, and the rectification column (33) increases the alcohol concentration of the raw alcohol to approximately 94 vol.%.
  3. System according to either claim 1 or claim 2, characterised in that the system is designed such that the rectification column (33) is operated at a head overpressure of up to 6 bar, and the rectified alcohol is supplied to the molecular sieve assembly (43) in vapour form.
  4. System according to any of claims 1 to 3, characterised in that a reboiler (139) which heats the intensifying column (19) is heated by dehydrogenated alcohol from the molecular sieve assembly (43).
  5. System according to claim 4, characterised in that the molecular sieve assembly (43) comprises at least two molecular sieves (101, 103, 105), of which, in cyclic permutation, at least one (101) receives the rectified alcohol in the drying mode and outputs the dehydrogenated alcohol by means of the reboiler (139) of the intensifying column (19), and of which at least a second (103, 105) of the molecular sieves receives a portion of the dehydrogenated alcohol in the regeneration mode and, by means of a condenser (109) and an evaporator (125), in particular a falling film evaporator, heated by means of live steam, supplies alcohol which has been moistened in the regeneration mode to the rectification column (33) as a flow to be rectified.
  6. System according to either claim 4 or claim 5, characterised in that a further reboiler (77) which heats the intensifying column (19) is heated by top vapour from the rectification column (33).
  7. System according to any of claims 4 to 6, characterised in that a reboiler (79) which heats the rectification column (33) is heated by live steam.
  8. System according to any of claims 4 to 7, characterised in that the reboiler (77) of the intensifying column (19) and/or the reboiler (79) of the rectification column (33) are formed as an evaporator, in particular a falling film evaporator, arranged in a forced circulation circuit (35, 83).
  9. System according to claim 8, characterised in that the forced circulation circuit (35) of the reboiler (77) of the intensifying column (19) is guided through the foot region (39) thereof, and the alcohol flow to the rectification column (33) is branched off from this forced circulation circuit (35).
  10. System according to either claim 8 or claim 9, characterised in that the condensate of the reboiler (27) of the distillation column (5) and/or the condensate of the reboiler (77) of the rectification column (19) can be supplied to the intensifying column (19) and/or the rectification column (33) as reflux.
  11. System according to claims 5 to 10, characterised in that the dehydrogenated alcohol downstream of the reboiler (139) of the intensifying column (19) preheats the condensed alcohol-water mixture from the condenser (109) in a heat exchanger (119).
  12. System according to any of claims 6 to 11, characterised in that the condensate of the reboiler (77) of the intensifying column (19), which reboiler is heated by the top vapour of the rectification column (33), can be supplied to the intensifying column (19) and/or the rectification column (33) as a return flow.
  13. System according to any of claims 1 to 12, characterised in that a reboiler (27) heated by the top vapour of the intensifying column (19) is associated with the distillation column (5), and the condensate of the top vapour of this reboiler (27) can be supplied to the intensifying column (19) and/or the rectification column (33) as reflux.
  14. System according to any of claims 1 to 13, characterised in that spent wash which accumulates in the distillation column (5) can be supplied to a separating device (51) which separates the spent wash into a solid fraction and a thin juice fraction, in that a reboiler which is formed as a falling film evaporator (27) and is heated by live steam or by top vapour from a column (19) which increases the alcohol concentration and is downstream in the product stream is associated with the distillation column (5) for the heating thereof, and at least part of the thin juice fraction is guided in a forced circulation circuit (47) through the falling film evaporator (27), and in that at least part of the thin juice fraction circulating in the forced circulation circuit (47) or vapours thereof can be supplied to the distillation column (5) for the heating thereof.
  15. System according to claim 14, characterised in that the falling film evaporator (27) is heated by the top vapour of an intensifying column (19) which is arranged in the alcohol product stream between the distillation column (5) and the rectification column (33) and increases the alcohol concentration of the raw alcohol.
  16. System according to any of claims 1 to 15, characterised in that raw alcohol vapour of the distillation column (5) can be at least partially condensed in an evaporator (55) used for generating steam, and the steam can be supplied, by means of a mechanical compressor (59) which increases the pressure and/or the temperature of the steam, to the distillation column (5) or to another distillation column, which draws off raw alcohol from the fermented mash, for the heating thereof.
  17. System according to claim 16, characterised in that the evaporator (55) is designed as a falling film evaporator.
  18. System according to claim 17, characterised in that the falling film evaporator for generating steam is arranged in a circulation circuit (63) for fresh water, spent wash or spent-wash vapours.
  19. System according to claim 18, characterised in that the mechanical compressor (59) is connected to the circulation circuit (63) by means of a separator (57) which separates the steam.
  20. System according to any of claims 16 to 19, characterised in that the mechanical compressor (59) comprises a plurality of mechanical compressor stages connected in series.
  21. System according to claims 16 to 20, characterised in that the distillation column (5) is heated by means of a reboiler (27) which is heated by means of the top vapour of a column connected downstream which increases alcohol concentration, in particular an intensifying column (19) arranged in the product stream between the distillation column (5) and the rectification column (33), and the distillation column is additionally heated by means of the compressed steam of the mechanical compressor (59).
EP07819126.9A 2006-10-18 2007-10-18 Installation for the distillation of alcohol, especially ethyl alcohol, from fermented mash Active EP2089130B1 (en)

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DE102006049173A DE102006049173A1 (en) 2006-10-18 2006-10-18 Plant for distilling alcohol, in particular ethyl alcohol from fermented mash
PCT/EP2007/009061 WO2008046634A1 (en) 2006-10-18 2007-10-18 Installation for the distillation of alcohol, especially ethyl alcohol, from fermented mash

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CN102716595A (en) * 2012-07-03 2012-10-10 宿州中粮生物化学有限公司 Control method of mash tower reboiler heat exchange in alcohol two-tower distilling device
DE102012217937A1 (en) * 2012-10-01 2014-04-03 Gea Wiegand Gmbh Plant for dealcoholizing an alcohol, in particular ethanol-containing product
CN103706141B (en) * 2014-01-22 2015-08-12 象山医疗精密仪器有限公司 Steam compression type alcohol distillation column and distillating method
DE102014222071A1 (en) * 2014-10-29 2016-05-04 Gea Wiegand Gmbh distillation plant
CN106966865B (en) * 2016-01-14 2023-07-04 天津市天地创智科技发展有限公司 System for treating glycine crystallization mother liquor by three-effect countercurrent evaporation rectification process
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CN108421274B (en) * 2017-10-30 2023-11-03 肥城金塔酒精化工设备有限公司 Low-pressure double-coarse double-fine eight-tower distillation device and method for preparing high-grade alcohol
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WO2008046634A1 (en) 2008-04-24
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BRPI0717520A2 (en) 2013-12-03
RU2421264C2 (en) 2011-06-20

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